Method of making diazo printing pastes and product



I E e'l'h t meet p r515 1 st t al DyQS fi B-I d dy Y- aratien: of emulsion printing pasltes off this type. althoughjtheircost 'js i'ather menses-many of Patented F eb. 2,1943

.w 7 53,319,913 I; enmzolram, .LJAQ ERO .e i Norman's;fiassliltiflsewood, niLIassigiieiteg,

t extile printing comms en ienel Daniel eie e s i resw and novel compositions useful the pi'eparation of textile printing pastes, and to iiieahsfofpre- M paring printing pastes therefrom.

In my copending application, Serial Number 215,585, tiled June 24, 1938, now-U. S. Patent No.

2,202,283, issued May 28, @1940, I have disclosed a means-whereby the disadvantages of conventional h I 1 i21rlnterchemicaliflorm a ni' w York il,

. .l a WNoDrawinLl-hzipplication G za-19st;

A; No.285,-969

acquer ni si n; ;'to.i -p id te a emulsi f olution ,of 'jdi'zo compound in a, continuous lla-aue tbh l 'ey ,frh e l o sem rorrami a nias .a iir e paste 5 er a paste byfthe "sii'njple dition' of t necessary ingredients."f-'=It{is thus possible' to "ec6i orr'iicallf produce 'a "printing paste just before printing; which presents no storage problems; .Thev diazotizable base may be dispersed in a textile printing pastes (such as poor printingfiio ivehiclefwli'iclr'has no solvent action thereon, or

inability to print from photogravure cylinders,

{be done. the 6.91%??? 95 .eshallow. en rav n s sm h the rteiltibnbf h complete deta l 9i 4 the. .EQ PQ IQW c9 1 and the use of a minimum tn jjh ,eiscioseaitms meahse qmll s; the vr na a a of dyestuil printing pastes by the emulsilflcation may be" dissolved in the vehicle: it is onlv' necessarythat the vehicle. be capable of emulsifying the water-in it. -I -;h ave disccvered that on treatment wan-masons acid u aj'friitrita theldiazotization of. the base mo ers-rapidly and smoothly. Where the salt orthe --base is water soluble it dissolves in the water globules and is thusiimade "available -for-rapid and-complete action in" small increments: whilethe insoluble salts are kept suscomponent with a water immiscible body'ing 'com- 7 nos t cn. (p efe abl a 3 1! 9 am el om substance in a solvent), the dyestuff solution beemulsionifl optimum;cqsfi. f iiat;ii i .o 4 applied to a fabric, as withla conventipnal intaglio cylinder; the dyestufi is flxed on the fabric, and

'heifabrici's'th'en dried, with or wi'thout washing, depending-orr thefdyestufiemp1oyed I, 1 J plied-meteemmsnm reverse the proclgcitufe, ffthejemuls'ion brel is, the'dyestiifis" solutionpene- As the mulsion'isinto the yarns" of the la-brie. Sinc'e the water pliase'fand jthe botlyln' g agent are mutually repellent; th 'non aqu'eous prevents undue spreading oi the aqueous phase. As a-resulhsub-e "ly'n flu occurfs, and fine printing is reserves-'fthe'fflne lines" ofa materials which gro ps are particularly useful in the prepfthem are stable on 'sto age'i stsiutionni water, 'evenwhen protected-by the emulsion? "I .have discovered}; simple means 'of economially preparing' emulsions containing diazu compounds My nv imqnconsists in'diazotiiin'g a Ldiazot'izable base in the presence of water which 5 tained.

estufl dampen neg containing? -40 reaction, so that u In most cases, Lprefento-add the aqueous acid ,sol tionto the emulsiflable'base, to form an emulsion of'the'soluble salt, ot the base befOre adding the nitrite; 1 However; it is sometimes desirable I e The diazotizable bases are preferably such T i a mp unds of-the class known r "5co1or salts; which co ple-withbases-of the class consisting of beta-oxy-naphthcic-acid" and it'sdedissolvedin the. aqueous phase,

If; the lacquer usedis tobe made into a textile ""is 'c'iispr'sed asthe innerfpha's of-"a wate'r'"-'in 50 printingpastedirectly'withouhfurther additlon of solvent or thickener, it is desirable that the lacquer have a low thickener content, so that the printing pastes made therefrom contain under about 5% thickener, and preferably a. much lower percentage. This low percentage of thickener permits of the production "of printing pastes in which the thickener need not be removed from the fabric. Since these .pastes ordinarily require at least 0.5% by weight of base, a ratio of 10 thickener to 1 diazotizable base should not in general be exceeded, if the material is to be used for printing after emulsification. I

Typical examples of my invention are the following:

Example 1 Parts by weigh BlueBBase (Dianisidine) 0.5

are added to a mixture of Allwd resin solution j 3.0 Pine nil v 5,0 Solvesso #3- (hydrogenated petroleum naphtha) (Boiling range 175-210 C.) 19.9

HC] (29 Tw.)

Water at 30 20.0

The emulsion formed is then cooled to about 0 to 0., and NaNO: 0.3

Water at 05 C 50.0

is emulsified into it. 1

Diazotization proceeds rapidly, along with emulsincation. The paste is ready for printine in about thirtyminutes; and may be appl ed to a fabric impre nated. for example, with the anilide of beta-oxy-naphthoic acid.

Example 2 Parts by weigh Dianisidine (Blue B Base) 0.5

is added to a solution of paste is then ready for printing.

EmmpteZ Parts by weight Scarlet RC Base (meta nitro ortho-anisi- After diazotization is complete (about so minutes) the whole is buflered with Parts by weight Sodium acetate 0.6

dissolved in Water 10.6

Example 4 Parts by weight Blue B B Base (4 benzoyl amino 3:8 diethoxy aniline) 4 NH: is added to an organic phase of Ethyl cellulose (250 centipoise) 0.8

Pine oil 3.0

Xylol r 8.2

Solvesso #3' 25.0

Into this is emulsified NaNOz 0.4

Water at 0-5 C 39.3

I and HCl (29 Tw.) 1.7

is then added. Diazotization is complete in 15-30 minutes.

Various changes in the examples can be made without departing from the scope ofthe invention, which is defined in the claims. While I have shown the invention as applicable to the preparation of textilgprinting pastes, it can, of course, be used wherever an emulsion of a diazotizable base solution is desirable.

I claim: l. The method of diazotizing a diazotizable base which comprises conducting the diazotization while the base is in contact with water which forms the inner phase of a water-in-oil emulsion. 2. The method of diazotizing a diazotizable base which comprises preparing a mixture of the base with a water immiscible liquid capable of emulsifying water therein. and adding aqueous fluid containing reactants which will cause diazotization of the base, whereby the base is diazotized and dissolved in the water to form an emulsion of a solution of a diazo compound in a continuous water immiscible phase.

Ethyl cellulose (250 centipoise) 0.8

xyini 8.2

Pine nil .3. 0

-Solvesso #3 a r 25.0

into this is emulsifled- '1 H01 (29 Tw.) 1.3

in a i 1 a Water at C .L. 20.0 this is'cooled to 0-5 C... and

NaNO: j .3

Cold water (J-5 C.) 30.0 is emuls fied in. after diazotization is complete, in 20 to 40 minutes Sodium acetate 0.4

dissolved in Water 1 4 11.0 is added to neutralize excess acid. The v 3. The method oLdiazotizing a diaz'otizable base which comprises preparing a mixture of the base with a water immiscible lacquer capable of emulsifying water therein, and adding aqueous fluid containing reactants which will cause diazotization of the base, whereby the base is. diazotized and dissolved in the water to form an emulsion of a solution of a diazo compound in a continuous water immiscible; lacquer phase.

4. The method of diazotizing a diazotizable base which comprises preparing a mixture of the base with a water immiscib e liquid bapflble of emulsifying water therein, adding'ah aqueous fluid in which the base is soluble, to form a waterin-oil emulsion, and thereafter addingto the emulsion and aqueous solution of chemical capable of reacting with the base to compounq.

form a diazo 15 wateb-in-oil emulsion.

.5. The method oi preparing a printing-paste for textile fabrics containing a; diazo compound,

which comprises preparingca mixture offa diazotizable base and a lacquer capable ofcemi lsiffing water therein, emulsifying an aqueous acici so: lution into the lacquer to produce an emulsion with the base in solution in the water. and-there;

after emulsifying: an aqueous solution ofa diagotizing agent into the emulsion.

s. The, method of 'diazotizing a dia'zotizable f base which comprises diazotizing the base with aqueous solutions of diazo'tiz'ation reactants while I n the aqueous solutions of the diazotization reactants are dispersed as the inner phase of a Noam s. CASSEL. 

